CN102234183A - Anti-reflection coating and super-hydrophobic self-cleaning anti-reflection coating and preparation method thereof - Google Patents
Anti-reflection coating and super-hydrophobic self-cleaning anti-reflection coating and preparation method thereof Download PDFInfo
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- CN102234183A CN102234183A CN2010101627464A CN201010162746A CN102234183A CN 102234183 A CN102234183 A CN 102234183A CN 2010101627464 A CN2010101627464 A CN 2010101627464A CN 201010162746 A CN201010162746 A CN 201010162746A CN 102234183 A CN102234183 A CN 102234183A
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- dimethyl ammoniumchloride
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Abstract
The invention relates to an anti-reflection coating and a super-hydrophobic self-cleaning anti-reflection coating and a preparation method thereof. The anti-reflection coating is formed by a SiO2 ball-shaped nanoparticle layer with the particle size of 10-100 nm, and the surface of the coating has a rough structure. The super-hydrophobic self-cleaning anti-reflection coating is formed by providing a low surface energy substance on the surface of the anti-reflection coating, and the surface of the low surface energy substance has a rough structure. The coatings are obtained by using layer-by-layer electrostatic self-assembly technique. The light transmittance of the glass coated with the super-hydrophobic self-cleaning anti-reflection coating can increase to 99.1 from 91.3%, and the single-side reflectivity of the glass can reduce lowest to 0.3%. Compared with a solar cell coated with a common glass flake, a standard mono-silicon solar cell panel coated with a glass with the super-hydrophobic self-cleaning anti-reflection coating can utilize solar energy more effectively, and the efficiency can be improved to more than 6.6%.
Description
Technical field
The invention belongs to the nano material preparation technical field, particularly anti-reflection coating of anti-reflection coating and super-hydrophobic automatic cleaning and its production and use.
Background technology
Automatically cleaning and anti-reflection nano-structured coating have in fields such as solar energy power generating, photovoltaic building material, solar energy collector, aerospace to be used and huge market widely.China only solar water heater just reaches 100,000,000 square metres to the demand of solar energy glass, expect the year two thousand thirty photovoltaic generation and be expected to account for 5%～20% of energy production world amount, in China, except Application Areas and science and technology demonstration, country's pilot project, project supported by commen people and international cooperative project, every township will have electricity, bright engineering, country is grid-connected etc. has all started, and the Application of Solar Energy technical research and demonstration base of Asia maximum is built up in the Yuzhong County, Gansu Province and put into operation.Can look forward to, one is utilized the New Times of sun power to arrive on a large scale.Solar energy glass will become sheet glass industry new growth engines, and it not only can drive the sheet glass industry restructuring, and can realize the Sustainable development of sheet glass industry.The extensive utilization of sun power needs higher transmittance and lower reflectivity, and big area is put into operation and brought very heavy cleaning simultaneously, presses for the surface and has self-cleaning function.At present, domestic coating research with super-hydrophobic automatic cleaning function and good anti-reflection performance is used also seldom.
Just begun the research of glass automatically cleaning and anti-reflection abroad in the sixties in 20th century, the anti-reflection layer adopts the homogeneous film of different refractivity to realize antireflective effect usually, according to the anti-reflection principle of present optics, thickness can have very narrow anti-reflection result at the single wavelength place when λ/4 places.If will realize the film of the just necessary stack multilayer of wide spectrum anti-reflection different media, this has brought difficulty for complete processing and technology.JP 10-20102A discloses a kind of anti-reflection film that comprises 7 layers of different media layer, but this anti-reflection film in the wavelength of about 400 nanometers and 700 nanometers to the anti-reflection performance deficiency of visible light.JP2006-3562 discloses and has a kind ofly comprised a plurality of layers anti-reflection film but the visible light near 400 nano wave lengths is not had enough reflectivity.And the present invention uses single nanoparticle layers to realize visible-range inner width spectrographic anti-reflection.Maximum transmission can be up to 99%, and the single face reflectivity is 0.3%.
At present, all there is renowned company in developed country in the research and development of specializing in self-cleaning glass and making in the world, as Britain Pilkington company, Japanese TOTO company, U.S. PPG company, German GEA company, VTA company, UIC company etc.; Aspect application and development, Japan takes the lead in launching exploitation, promotes, uses TiO
2The photochemical catalysis self-cleaning glass.Britain Pilkington glass company is at Application and Development TiO
2Photocatalytic self-cleaning glass aspect has been walked the prostatitis the glass merchant of Europe, the United States.Transparent composite self-cleaning antifog glass (W.L.Tonar et al.Electrochromic DeviceHaving A Self-cleaning Hydrophilic Coating.United States Patent ApplicationPublication US2001/00210066 A1, the 2001-09-13 of people such as U.S. W.L.Tonar development; K.Toru.Vehicle Mirror.United States Patent US5594585:1997-01-14; K.Toru.Anti-fog Element.US5854708:1998-12-29; K.Takahama et al.Method of Forming HydrophilicInorganic Coating Film And Inorganic Coating Composition.United States PatentApplication Publication US2001/008696 A1,2001-07-13), be to form photocatalyst Clear coating, form the transparent porous inorganic oxide (SiO of possess hydrophilic property again on the surface of photocatalyst Clear coating with katalysis on the surface of glass baseplate
2And Al
2O
3) film.Yet these technology have all been utilized TiO
2Photocatalysis characteristic impels the surface to reach super hydrophilic, and applicable elements can be restricted, and just can carry out katalysis because need the environment of illumination; Though and this cavernous structure surface can improve wetting ability, be easy to be killed in a disaster evaporable material or nanometer dust are blocked the aperture, and weather resistance is undesirable.
The present invention has adopted SiO
2Colloidal sol self-assembly layer by layer prepares the anti-reflection coating, further carries out hydrophobization and handles its surface, preparation super-hydrophobic automatic cleaning anti-reflection coating.Described super-hydrophobic automatic cleaning anti-reflection coating has very high water contact angle, and water droplet drops in the surface can form spheroid, is easy to tumble take away pollutent and do not stay any vestige, thereby realizes self-cleaning ability.
Substrate can be a sheet glass, and for example, the glass window of family and commercial building, glass sunroof, glass curtain wall, Household bathroom mirror, windshield, rear vision mirror, background glass, eye plate etc. also can be flexible polymer films.SiO
2The nanoparticle iso-electric point is greatly about 2.1, and the surface easily shows electronegativity, is easy to be adsorbed on the substrate of positively charged polyelectrolyte modification.Utilize this electrostatic force can realize Layer-by-Layer (LBL) self-assembly layer by layer.Formed the kapillary nerve of a covering on the coating base plate surface of nano SiO 2 particle, and its surface there is abundant-Si-OH group, can improves its weather resistance widely, can form cancellated coating attached to body surface securely.Formed silicon dioxide granule can increase frictional coefficient, thereby has certain wearability, and silicon-dioxide also has lower reflectivity and good wear resistance energy in addition.The transmittance that scribbles the sheet glass of super-hydrophobic automatic cleaning anti-reflection coating can bring up to 99.1% from 91.3%, and the single face reflectivity is minimum to drop to 0.3%.The sheet glass of super-hydrophobic automatic cleaning anti-reflection coating of the present invention covers on the standard single-crystalline-silicon solar-cell panel, and the solar cell of comparing the covering of simple glass sheet more can effectively utilize solar energy, and battery efficiency improves more than 6.6%.
Summary of the invention
One of purpose of the present invention provides the anti-reflection coating that the surface has coarse structure.
Two of purpose of the present invention provides the super-hydrophobic automatic cleaning anti-reflection coating that the surface has coarse structure, and the transmittance that scribbles the sheet glass of this coating can bring up to 99.1% from 91.3%.
Three of purpose of the present invention provides and adopts the static self-assembling method, and nanoparticle and polyelectrolyte are replaced assembling, thereby the preparation method of preparation method and the anti-reflection coating that technology is simple, raw material is cheap, cost is low, applied widely is provided.
Four of purpose of the present invention provides the preparation method that the surface has the super-hydrophobic automatic cleaning anti-reflection coating of coarse structure.
Anti-reflection coating of the present invention is the SiO that is approximately 10～100nm by particle diameter
2The nano spherical particle layer constitutes, and the surface of this anti-reflection coating has coarse structure.
The anti-reflection coating of super-hydrophobic automatic cleaning of the present invention is at the SiO that is approximately 10～100nm by particle diameter
2There is a layered low-surface energy material on the surface of the anti-reflection coating that the nano spherical particle layer constitutes, and the surface of low surface energy material layer has coarse structure.
Described low surface energy material is selected from a kind of in trifluoro propyl Trimethoxy silane, trifluoro propyl triethoxyl silane, ten trifluoro octyl group Trimethoxy silanes, ten trifluoro octyltri-ethoxysilane, 17 fluorine decyl Trimethoxy silanes, 17 fluorine decyl triethoxyl silanes, the ten difluoro heptyl propyl trimethoxy silicanes etc.
Anti-reflection coating of the present invention is to adopt the prepare suspension of commercially available or own synthetic Nano particles of silicon dioxide, takes dip-coating method SiO
2Nano spherical particle and polyelectrolyte deposit on the substrate (as sheet glass) by the static assembling, prepare the anti-reflection coating through calcining at last, further carry out obtaining after hydrophobization is handled the anti-reflection coating of super-hydrophobic automatic cleaning.Required plant and instrument is simple, cheap, is easy to industrialization.
Described particle diameter is approximately the SiO of 10～100nm
2Nano spherical particle is desirable commercially available, or according to
(
W, Fink A, Bohn E.Journal of Colloid ﹠amp; Interface Science, 1968,26:62～69) method is prepared.
Coating described in the present invention is to pass through SiO
2On the negative charge of nano spherical particle surface band and the substrate sedimentary polyelectrolyte with positive charge the electrostatic attraction self-assembly and form, each step finishes and all thoroughly washs with distilled water, dries up with rare gas element (as nitrogen).
Described polyelectrolyte is diallyl dimethyl ammoniumchloride and sodium polystyrene sulfonate.
The preparation method of anti-reflection coating of the present invention may further comprise the steps:
(1) processing substrate is clean, remove surface contaminant;
(2) substrate that obtains after step (1) is dried up with rare gas element (as nitrogen) is immersed in the aqueous solution of diallyl dimethyl ammoniumchloride that concentration is 1～3mg/mL and takes out after 2～10 minutes, in substrate surface deposition one deck diallyl dimethyl ammoniumchloride coating,, dry up to remove the diallyl dimethyl ammoniumchloride of physical adsorption with distilled water wash with rare gas element (as nitrogen); And then be immersed in the sodium polystyrene sulfonate aqueous solution that concentration is 1～3mg/mL 2～10 minutes, take out, use distilled water wash, dry up, on the diallyl dimethyl ammoniumchloride coating, deposit one deck sodium polystyrene sulfonate coating again with rare gas element (as nitrogen); Repeat the processing step of above-mentioned deposition diallyl dimethyl ammoniumchloride coating and sodium polystyrene sulfonate coating, until being deposited 5～20 layers of bilayer that constitutes by diallyl dimethyl ammoniumchloride coating and sodium polystyrene sulfonate coating altogether, and then repeat the processing step of above-mentioned deposition diallyl dimethyl ammoniumchloride coating, obtain the substrate that sedimentary last one deck is the diallyl dimethyl ammoniumchloride coating on substrate;
(3) last one deck that step (2) is prepared is that the substrate of diallyl dimethyl ammoniumchloride coating is immersed in and contains the SiO that particle diameter is approximately 10～100nm
2In the alcohol suspension of nano spherical particle 2～10 minutes, take out and use distilled water wash, rare gas element (as nitrogen) dries up, and deposits one deck SiO at the diallyl dimethyl ammoniumchloride coatingsurface
2The nano spherical particle layer; And then be immersed in taking-up after 2～10 minutes in the diallyl dimethyl ammoniumchloride aqueous solution that concentration is 1～3mg/mL, at SiO
2Nano spherical particle laminar surface deposition one deck diallyl dimethyl ammoniumchloride coating, dries up with rare gas element (as nitrogen) to remove the diallyl dimethyl ammoniumchloride of physical adsorption with distilled water wash; Repeat above-mentioned deposition SiO
2The processing step of nano spherical particle layer and deposition diallyl dimethyl ammoniumchloride coating, until the last one deck that obtains in step (2) is on the substrate of diallyl dimethyl ammoniumchloride coating, is deposited 2～14 layers of SiO that is approximately 10～100nm by particle diameter altogether
2The bilayer that nano spherical particle layer and diallyl dimethyl ammoniumchloride coating constitute, and then repeat above-mentioned deposition SiO
2The processing step of nano spherical particle layer obtains that sedimentary last one deck is the SiO that particle diameter is approximately 10～100nm on substrate
2The substrate of nano spherical particle layer;
(4) outermost layer that step (3) is prepared is SiO
2The substrate of nano spherical particle layer is put into retort furnace, is 500～600 degrees centigrade of following sintering (preferred sintering time is 2～5 hours) in temperature, to remove polyelectrolyte diallyl dimethyl ammoniumchloride and sodium polystyrene sulfonate, has strengthened SiO simultaneously
2The sticking power of nano spherical particle and substrate obtains anti-reflection coating of the present invention on substrate.
Step (3) is described to contain the SiO that particle diameter is 10～100nm
2The mass concentration of the alcohol suspension of nano spherical particle is 0.1%～1%.
The preparation method of super-hydrophobic automatic cleaning anti-reflection coating of the present invention is:
The substrate that has the anti-reflection coating that method for preparing obtains is put into the container (as polytetrafluoroethylcontainer container) of sealing, in container, add an amount of low surface energy material, and the liquid level that makes the low surface energy material that is added is lower than the bottom of described substrate, in temperature is to make the evaporation of low surface energy material under 100～500 degrees centigrade, the hydatogenesis of low surface energy material on the anti-reflection coating that has prepared, is finally obtained super-hydrophobic automatic cleaning anti-reflection coating on substrate.
The processing of the described substrate of step (1) can for: it is 98% H that substrate is immersed in mass concentration
2SO
4With mass concentration be 30% H
2O
2Be in 7: 3 blended mixed solutions by volume, take out and use distilled water wash, dry up with rare gas element (as nitrogen); Perhaps used the oxygen plasma treatment surface 5～15 minutes.
Described low surface energy material is selected from a kind of in trifluoro propyl Trimethoxy silane, trifluoro propyl triethoxyl silane, ten trifluoro octyl group Trimethoxy silanes, ten trifluoro octyltri-ethoxysilane, 17 fluorine decyl Trimethoxy silanes, 17 fluorine decyl triethoxyl silanes, ten difluoro heptyl propyl trimethoxy silicanes, the hexafluoro butyl propyl trimethoxy silicane etc.
Described substrate is a sheet glass, for example, and the glass window of family and commercial building, glass sunroof, glass curtain wall, Household bathroom mirror, windshield, automobile rearview mirror, automobile background glass or eye plate etc.
The present invention with the cheap and sheet glass easily obtained as substrate, again by layer upon layer electrostatic self-assembly deposition charged polyelectrolytes and SiO
2Nano spherical particle.Because SiO
2The increase of the porosity between the nano spherical particle makes the transmittance of the sheet glass that scribbles super-hydrophobic automatic cleaning anti-reflection coating bring up to 99.1% from 91.3%, and the single face reflectivity is minimum to drop to 0.3%.
Super-hydrophobic automatic cleaning anti-reflection coating of the present invention is the SiO that has utilized in the anti-reflection coating that is made of the nano spherical particle layer of the present invention
2The surface has good hydrophilicity and silica membrane and has advantages such as low luminous reflectance factor, high light transmission rate, wear resisting property be good, in conjunction with coatingsurface by SiO
2The rough surface structure that nanoparticle constitutes is further modified the low surface energy material and is made described anti-reflection coating have ultra-hydrophobicity, and water is spent near 150 at the contact angle of the glass surface that scribbles this coating.When water droplet drops on the glass surface that scribbles this coating, can form the globule, be easy to tumble and get off to take away surface contaminant, realize self-cleaning function.This coating among the present invention has technical superioritys such as preparation technology is simple, cost is low, effect is obvious, applied widely.The sheet glass of super-hydrophobic automatic cleaning anti-reflection coating of the present invention covers on the standard single-crystalline-silicon solar-cell panel, and the solar cell of comparing the covering of simple glass sheet more can effectively utilize solar energy, and battery efficiency improves more than 6.6%.
The present invention is further illustrated below in conjunction with drawings and Examples, and wherein (S-20) in the accompanying drawing is the SiO of particle diameter 10～30nm
2Nano spherical particle, the following coat layer number that is designated as that bracket is outer.
Description of drawings
Fig. 1. (a) the depositing of the embodiment of the invention 1 (S-20)
1The sem photograph of the sheet glass of coating; (b) be cross-sectional view; The following coat layer number that is designated as that bracket is outer.
Fig. 2. (a) the depositing of the embodiment of the invention 2 (S-20)
4The scanning electron microscope picture of the sheet glass of coating (b) is the amplification picture of (a); The following coat layer number that is designated as that bracket is outer.
Fig. 3. (a) the depositing of the embodiment of the invention 3 (S-20)
8The scanning electron microscope picture of the sheet glass of coating (b) is the amplification picture of (a); The following coat layer number that is designated as that bracket is outer.
Fig. 4. (a) the depositing of the embodiment of the invention 4 (S-20)
9The scanning electron microscope picture of the sheet glass of coating (b) is the amplification picture of (a); The following coat layer number that is designated as that bracket is outer.
Fig. 5. (a) the depositing of the embodiment of the invention 5 (S-20)
10The scanning electron microscope picture of the sheet glass of coating (b) is the amplification picture of (a); The following coat layer number that is designated as that bracket is outer.
Fig. 6. deposit (S-20)
nThe transmittance of the sheet glass of coating; N is 0,1,4,8,9,10, and 0 among the figure, 1,4,8,9,10 lines are corresponding respectively not to have the transmittance of the sample of the glass substrate of coating, embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5.The following coat layer number that is designated as that bracket is outer.
Fig. 7. deposit (S-20)
nThe reflectivity of the sheet glass of coating: n is 0,1,4,8,9,10, and 0 among the figure, 1,4,8,9,10 lines are corresponding respectively not to have the reflectivity of the sample of the glass substrate of coating, embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5.The following coat layer number that is designated as that bracket is outer.
Fig. 8. deposit (S-20)
9Sheet glass of coating (embodiment 4) and clean simple glass sheet contrast photo, the left side is the simple glass sheet, has obviously reflective; The right is for depositing (S-20)
9The sheet glass of coating.
Fig. 9. deposit (S-20)
9Sheet glass of coating (embodiment 4) and clean simple glass sheet contrast photo, it is reflective that last figure simple glass sheet has been faced tangible mirror image, and the sheet glass of anti-reflection coating does not have, still like this behind figure below reversing of position.
Figure 10. (a) Jie Jing simple glass sheet and (b) deposit (S-20)
8The water contact angle photo of the sheet glass of coating (embodiment 3).
Embodiment
Antireflecting coating: by one deck particle diameter is the SiO of 10～30nm
2Nanoparticle is formed, and its preparation method may further comprise the steps:
(1) with 3-6mL ammoniacal liquor, the 50-150mL dehydrated alcohol added in the Erlenmeyer flask stirring at normal temperature 8-12 minute, stirred 1-3 minute at 50-70 degree centigrade, under agitation drip 2-4mL tetraethoxy (TEOS), at 50-70 degree centigrade of vigorous stirring 10-14 hour, obtain translucent suspension, gained contains the SiO that diameter is 10～30nm
2Nano spherical particle suspension, and to be diluted to massfraction be that 0.1%～1% suspension is standby;
(2) (mass concentration is about 98% H the simple glass sheet to be immersed the Pirhana solution of newly joining
2SO
4Be about 30% H with mass concentration
2O
2Be 7: 3 blended mixed solutions by volume) 5～20 minutes, take out and use distilled water wash, dry up with nitrogen;
(3) sheet glass after step (2) is dried up with nitrogen is immersed in the diallyl dimethyl ammoniumchloride aqueous solution that concentration is 1～3mg/mL and takes out after 2～10 minutes, in glass surface deposition one deck diallyl dimethyl ammoniumchloride coating,, dry up to remove the diallyl dimethyl ammoniumchloride of physical adsorption with distilled water wash with nitrogen; And then immersed in the sodium polystyrene sulfonate aqueous solution that concentration is 1～3mg/mL 2～10 minutes, take out, use distilled water wash, dry up with nitrogen, on the diallyl dimethyl ammoniumchloride coating, deposit one deck sodium polystyrene sulfonate coating again; Repeat the processing step of above-mentioned deposition diallyl dimethyl ammoniumchloride coating and sodium polystyrene sulfonate coating, until being deposited 5 bilayers that constitute by diallyl dimethyl ammoniumchloride coating and sodium polystyrene sulfonate coating altogether, and then be immersed in the diallyl dimethyl ammoniumchloride aqueous solution that concentration is 1～3mg/mL after 2～10 minutes and take out,, dry up to remove the diallyl dimethyl ammoniumchloride of physical adsorption with distilled water wash with nitrogen; Obtain the sheet glass that sedimentary last one deck is the diallyl dimethyl ammoniumchloride coating on sheet glass;
(4) last one deck that step (3) is prepared is that the sheet glass of diallyl dimethyl ammoniumchloride coating is immersed in step (1) and contains the SiO that particle diameter is 10～30nm
2In the suspension of nano spherical particle 2～10 minutes, take out and use distilled water wash, nitrogen dries up, and deposits one deck SiO at the diallyl dimethyl ammoniumchloride coatingsurface
2Nanoparticle layers, depositing 1 is the SiO of 10～30nm by particle diameter
2The bilayer that nano spherical particle layer and diallyl dimethyl ammoniumchloride coating constitute;
(5) with step (4) preparation with SiO
2The sheet glass of nanoparticle coating is put into retort furnace, and 500～600 degrees centigrade of sintering 2～5 hours, to remove polyelectrolyte diallyl dimethyl ammoniumchloride and sodium polystyrene sulfonate, obtaining by the individual layer particle diameter was the SiO of 10～30nm
2The surface that the nano spherical particle layer constitutes has the anti-reflection coating of coarse structure;
(6) glass substrate of step (5) preparation is put into the polytetrafluoroethylcontainer container of sealing, add an amount of ten trifluoro octyl group Trimethoxy silanes, and the liquid level that makes the ten trifluoro octyl group Trimethoxy silanes that added is lower than the bottom of described glass substrate, in temperature is to make ten trifluoro octyl group Trimethoxy silane thermal evaporations under 100～150 degrees centigrade, ten trifluoro octyl group Trimethoxy silane thermal evaporations are deposited on the above-mentioned anti-reflection coating, finally obtain super-hydrophobicity automatically cleaning anti-reflection coating, it is to be the SiO of 10～30nm by particle diameter
2There are one deck ten trifluoro octyl group Trimethoxy silanes on the surface of the anti-reflection coating that the nano spherical particle layer constitutes, and the surface of ten trifluoro octyl group Trimethoxy silanes has coarse structure.The surface of the anti-reflection coating of described super-hydrophobic automatic cleaning and cross section pattern are as shown in Figure 1.Coat-thickness is about 25nm, and transmittance is shown in Fig. 6 center line 1.Reflectivity is shown in Fig. 7 center line 1.
Embodiment 2
Antireflecting coating: by four layers of particle diameter SiO that is 10～30nm
2Nanoparticle is formed, and its preparation method may further comprise the steps:
(1) with 3-6mL ammoniacal liquor, the 50-150mL dehydrated alcohol added in the Erlenmeyer flask stirring at normal temperature 8-12 minute, stirred 1-3 minute at 50-70 degree centigrade, under agitation drip 2-4mL tetraethoxy (TEOS), continue to stir 10-14 hour at 50-70 degree centigrade, obtain translucent suspension, gained contains the SiO that diameter is 10～30nm
2Nano spherical particle suspension, and to be diluted to massfraction be that 0.1%～1% suspension is standby;
(2) (mass concentration is about 98% H the simple glass sheet to be immersed the Pirhana solution of newly joining
2SO
4Be about 30% H with mass concentration
2O
2Be 7: 3 blended mixed solutions by volume) 5～20 minutes, take out and use distilled water wash, dry up with nitrogen;
(3) sheet glass after step (2) is dried up with nitrogen is immersed in the diallyl dimethyl ammoniumchloride aqueous solution that concentration is 1～3mg/mL and takes out after 2～10 minutes, in glass surface deposition one deck diallyl dimethyl ammoniumchloride coating,, dry up to remove the diallyl dimethyl ammoniumchloride of physical adsorption with distilled water wash with nitrogen; And then immersed in the sodium polystyrene sulfonate aqueous solution that concentration is 1～3mg/mL 2～10 minutes, take out, use distilled water wash, dry up with nitrogen, on the diallyl dimethyl ammoniumchloride coating, deposit one deck sodium polystyrene sulfonate coating again; Repeat the processing step of above-mentioned deposition diallyl dimethyl ammoniumchloride coating and sodium polystyrene sulfonate coating, until being deposited 10 bilayers that constitute by diallyl dimethyl ammoniumchloride coating and sodium polystyrene sulfonate coating altogether, and then repeat the processing step of above-mentioned deposition diallyl dimethyl ammoniumchloride coating, obtain the sheet glass that sedimentary last one deck is the diallyl dimethyl ammoniumchloride coating on sheet glass;
(4) last one deck that step (3) is prepared is that the sheet glass of diallyl dimethyl ammoniumchloride coating is immersed in step (1) and contains the SiO that particle diameter is 10～30nm
2In the suspension of nano spherical particle 2～10 minutes, take out and use distilled water wash, nitrogen dries up, and deposits one deck SiO at the diallyl dimethyl ammoniumchloride coatingsurface
2Nanoparticle layers, and then be immersed in taking-up after 2～10 minutes in the diallyl dimethyl ammoniumchloride aqueous solution that concentration is 1～3mg/mL, at SiO
2Nanoparticle layers surface deposition one deck diallyl dimethyl ammoniumchloride coating, dries up with nitrogen to remove the diallyl dimethyl ammoniumchloride of physical adsorption with distilled water wash; Repeat above-mentioned deposition SiO
2The processing step of nanoparticle layers and deposition diallyl dimethyl ammoniumchloride coating is the SiO of 10～30nm until depositing 3 altogether by particle diameter
2The bilayer that nano spherical particle layer and diallyl dimethyl ammoniumchloride coating constitute, and then repeat above-mentioned deposition SiO
2The processing step of nano spherical particle layer obtains that sedimentary last one deck is that particle diameter is the SiO of 10～30nm on sheet glass
2The sheet glass of nano spherical particle layer;
(5) with step (4) preparation with SiO
2The sheet glass of nanoparticle coating is put into retort furnace, 500～600 degrees centigrade of sintering 2～5 hours, and to remove polyelectrolyte diallyl dimethyl ammoniumchloride and sodium polystyrene sulfonate, the SiO that to obtain by four layers of particle diameter be 10～30nm
2The surface that the nano spherical particle layer constitutes has the antireflecting coating of coarse structure;
(6) glass substrate of step (5) preparation is put into the polytetrafluoroethylcontainer container of sealing, add an amount of ten trifluoro octyl group Trimethoxy silanes, and the liquid level that makes the ten trifluoro octyl group Trimethoxy silanes that added is lower than the bottom of described glass substrate, in temperature is to make ten trifluoro octyl group Trimethoxy silane thermal evaporations under 100～150 degrees centigrade, ten trifluoro octyl group Trimethoxy silane thermal evaporations are deposited on the above-mentioned anti-reflection coating, finally obtain super-hydrophobicity automatically cleaning anti-reflection coating, it is to be the SiO of 10～30nm by particle diameter
2There are one deck ten trifluoro octyl group Trimethoxy silanes on the surface of the anti-reflection coating that the nano spherical particle layer constitutes, and the surface of ten trifluoro octyl group Trimethoxy silanes has coarse structure.The surface of the anti-reflection coating of described super-hydrophobic automatic cleaning and cross section pattern are as shown in Figure 2.Coat-thickness is about 43nm, and transmittance is shown in Fig. 6 center line 4.Reflectivity is shown in Fig. 7 center line 4.
Embodiment 3
Antireflecting coating: by eight layers of particle diameter SiO that is 10～30nm
2Nanoparticle is formed, and its preparation method may further comprise the steps:
(1) with 3-6mL ammoniacal liquor, the 50-150mL dehydrated alcohol added in the Erlenmeyer flask stirring at normal temperature 8-12 minute, stirred 1-3 minute at 50-70 degree centigrade, under agitation drip 2-4mL tetraethoxy (TEOS), continue to stir 10-14 hour at 50-70 degree centigrade, obtain translucent suspension, gained contains the SiO that diameter is 10～30nm
2Nano spherical particle suspension, and to be diluted to massfraction be that 0.1%～1% suspension is standby;
(2) (mass concentration is about 98% H the simple glass sheet to be immersed the Pirhana solution of newly joining
2SO
4Be about 30% H with mass concentration
2O
2Be 7: 3 blended mixed solutions by volume) 5～20 minutes, take out and use distilled water wash, dry up with nitrogen;
(3) sheet glass after step (2) is dried up with nitrogen is immersed in the diallyl dimethyl ammoniumchloride aqueous solution that concentration is 1～3mg/mL and takes out after 2～10 minutes, in glass surface deposition one deck diallyl dimethyl ammoniumchloride coating,, dry up to remove the diallyl dimethyl ammoniumchloride of physical adsorption with distilled water wash with nitrogen; And then immersed in the sodium polystyrene sulfonate aqueous solution that concentration is 1～3mg/mL 2～10 minutes, take out, use distilled water wash, dry up with nitrogen, on the diallyl dimethyl ammoniumchloride coating, deposit one deck sodium polystyrene sulfonate coating again; Repeat the processing step of above-mentioned deposition diallyl dimethyl ammoniumchloride coating and sodium polystyrene sulfonate coating, until being deposited 10 bilayers that constitute by diallyl dimethyl ammoniumchloride coating and sodium polystyrene sulfonate coating altogether, and then repeat the processing step of above-mentioned deposition diallyl dimethyl ammoniumchloride coating, obtain the sheet glass that sedimentary last one deck is the diallyl dimethyl ammoniumchloride coating on sheet glass;
(4) last one deck that step (3) is prepared is that the sheet glass of diallyl dimethyl ammoniumchloride coating is immersed in step (1) and contains the SiO that particle diameter is 10～30nm
2In the suspension of nano spherical particle 2～10 minutes, take out and use distilled water wash, nitrogen dries up, and deposits one deck SiO at the diallyl dimethyl ammoniumchloride coatingsurface
2Nanoparticle layers, and then be immersed in taking-up after 2～10 minutes in the diallyl dimethyl ammoniumchloride aqueous solution that concentration is 1～3mg/mL, at SiO
2Nanoparticle layers surface deposition one deck diallyl dimethyl ammoniumchloride coating, dries up with nitrogen to remove the diallyl dimethyl ammoniumchloride of physical adsorption with distilled water wash; Repeat above-mentioned deposition SiO
2The processing step of nanoparticle layers and deposition diallyl dimethyl ammoniumchloride coating is the SiO of 10～30nm until depositing 7 altogether by particle diameter
2The bilayer that nano spherical particle layer and diallyl dimethyl ammoniumchloride coating constitute, and then repeat above-mentioned deposition SiO
2The processing step of nano spherical particle layer obtains that sedimentary last one deck is that particle diameter is the SiO of 10～30nm on sheet glass
2The sheet glass of nano spherical particle layer;
(5) with step (4) preparation with SiO
2The sheet glass of nanoparticle coating is put into retort furnace, 500～600 degrees centigrade of sintering 2～5 hours, and to remove polyelectrolyte diallyl dimethyl ammoniumchloride and sodium polystyrene sulfonate, the SiO that to obtain by eight layers of particle diameter be 10～30nm
2The surface that the nano spherical particle layer constitutes has the antireflecting coating of coarse structure;
(6) glass substrate of step (5) preparation is put into the polytetrafluoroethylcontainer container of sealing, add an amount of ten trifluoro octyl group Trimethoxy silanes, and the liquid level that makes the ten trifluoro octyl group Trimethoxy silanes that added is lower than the bottom of described glass substrate, in temperature is to make ten trifluoro octyl group Trimethoxy silane thermal evaporations under 100～150 degrees centigrade, ten trifluoro octyl group Trimethoxy silane thermal evaporations are deposited on the above-mentioned anti-reflection coating, finally obtain super-hydrophobicity automatically cleaning anti-reflection coating, it is to be the SiO of 10～30nm by particle diameter
2There are one deck ten trifluoro octyl group Trimethoxy silanes on the surface of the anti-reflection coating that the nano spherical particle layer constitutes, and the surface of ten trifluoro octyl group Trimethoxy silanes has coarse structure.The surface of the anti-reflection coating of described super-hydrophobic automatic cleaning and cross section pattern are as shown in Figure 3.Coat-thickness is about 120nm, and transmittance is shown in Fig. 6 center line 8.Reflectivity is shown in Fig. 7 center line 8.Clean simple glass sheet and deposit (S-20)
8The water contact angle photo of the sheet glass of coating is as (a) among Figure 10 with (b).
Antireflecting coating: by nine layers of particle diameter SiO that is 10～30nm
2Nanoparticle is formed, and its preparation method may further comprise the steps:
(1) with 3-6mL ammoniacal liquor, the 50-150mL dehydrated alcohol added in the Erlenmeyer flask stirring at normal temperature 8-12 minute, stirred 1-3 minute at 50-70 degree centigrade, under agitation drip 2-4mL tetraethoxy (TEOS), continue to stir 10-14 hour at 50-70 degree centigrade, obtain translucent suspension, gained contains the SiO that diameter is 10～30nm
2Nano spherical particle suspension, and to be diluted to massfraction be that 0.1%～1% suspension is standby;
(2) (mass concentration is about 98% H the simple glass sheet to be immersed the Pirhana solution of newly joining
2SO
4Be about 30% H with mass concentration
2O
2Be 7: 3 blended mixed solutions by volume) 5～20 minutes, take out and use distilled water wash, dry up with nitrogen;
(3) sheet glass after step (2) is dried up with nitrogen is immersed in the diallyl dimethyl ammoniumchloride aqueous solution that concentration is 1～3mg/mL and takes out after 2～10 minutes, in glass surface deposition one deck diallyl dimethyl ammoniumchloride coating,, dry up to remove the diallyl dimethyl ammoniumchloride of physical adsorption with distilled water wash with nitrogen; And then immersed in the sodium polystyrene sulfonate aqueous solution that concentration is 1～3mg/mL 2～10 minutes, take out, use distilled water wash, dry up with nitrogen, on the diallyl dimethyl ammoniumchloride coating, deposit one deck sodium polystyrene sulfonate coating again; Repeat the processing step of above-mentioned deposition diallyl dimethyl ammoniumchloride coating and sodium polystyrene sulfonate coating, until being deposited 10 bilayers that constitute by diallyl dimethyl ammoniumchloride coating and sodium polystyrene sulfonate coating altogether, and then repeat the processing step of above-mentioned deposition diallyl dimethyl ammoniumchloride coating, obtain the sheet glass that sedimentary last one deck is the diallyl dimethyl ammoniumchloride coating on sheet glass;
(4) last one deck that step (3) is prepared is that the sheet glass of diallyl dimethyl ammoniumchloride coating is immersed in step (1) and contains the SiO that particle diameter is 10～30nm
2In the suspension of nano spherical particle 2～10 minutes, take out and use distilled water wash, nitrogen dries up, and deposits one deck SiO at the diallyl dimethyl ammoniumchloride coatingsurface
2Nanoparticle layers, and then be immersed in taking-up after 2～10 minutes in the diallyl dimethyl ammoniumchloride aqueous solution that concentration is 1～3mg/mL, at SiO
2Nanoparticle layers surface deposition one deck diallyl dimethyl ammoniumchloride coating, dries up with nitrogen to remove the diallyl dimethyl ammoniumchloride of physical adsorption with distilled water wash; Repeat above-mentioned deposition SiO
2The processing step of nanoparticle layers and deposition diallyl dimethyl ammoniumchloride coating is the SiO of 10～30nm until depositing 8 altogether by particle diameter
2The bilayer that nano spherical particle layer and diallyl dimethyl ammoniumchloride coating constitute, and then repeat above-mentioned deposition SiO
2The processing step of nano spherical particle layer obtains that sedimentary last one deck is that particle diameter is the SiO of 10～30nm on sheet glass
2The sheet glass of nano spherical particle layer;
(5) with step (4) preparation with SiO
2The sheet glass of nanoparticle coating is put into retort furnace, 500～600 degrees centigrade of sintering 2～5 hours, and to remove polyelectrolyte diallyl dimethyl ammoniumchloride and sodium polystyrene sulfonate, the SiO that to obtain by nine layers of particle diameter be 10～30nm
2The surface that the nano spherical particle layer constitutes has the antireflecting coating of coarse structure;
(6) glass substrate of step (5) preparation is put into the polytetrafluoroethylcontainer container of sealing, add an amount of ten trifluoro octyl group Trimethoxy silanes, and the liquid level that makes the ten trifluoro octyl group Trimethoxy silanes that added is lower than the bottom of described glass substrate, in temperature is to make ten trifluoro octyl group Trimethoxy silane thermal evaporations under 100～150 degrees centigrade, ten trifluoro octyl group Trimethoxy silane thermal evaporations are deposited on the above-mentioned anti-reflection coating, finally obtain super-hydrophobicity automatically cleaning anti-reflection coating, it is to be the SiO of 10～30nm by particle diameter
2There are one deck ten trifluoro octyl group Trimethoxy silanes on the surface of the anti-reflection coating that the nano spherical particle layer constitutes, and the surface of ten trifluoro octyl group Trimethoxy silanes has coarse structure.The surface of the anti-reflection coating of described super-hydrophobic automatic cleaning and cross section pattern are as shown in Figure 4.Coat-thickness is about 122nm, and transmittance is shown in Fig. 6 center line 9.Reflectivity is shown in Fig. 7 center line 9.Cated sheet glass and clean simple glass sheet contrast photo such as Fig. 8 and shown in Figure 9.In Fig. 9, it is reflective that simple glass sheet (left side) has been faced tangible mirror image, and have the sheet glass (right side) of anti-reflection coating not have, behind the reversing of position still so (figure below).
Embodiment 5
Antireflecting coating: by ten layers of particle diameter SiO that is 10～30nm
2Nanoparticle is formed, and its preparation method may further comprise the steps:
(1) with 3-6mL ammoniacal liquor, the 50-150mL dehydrated alcohol added in the Erlenmeyer flask stirring at normal temperature 8-12 minute, stirred 1-3 minute at 50-70 degree centigrade, under agitation drip 2-4mL tetraethoxy (TEOS), continue to stir 10-14 hour at 50-70 degree centigrade, obtain translucent suspension, gained contains the SiO that diameter is 10～30nm
2Nano spherical particle suspension, and to be diluted to massfraction be that 0.1%～1% suspension is standby;
(2) (mass concentration is about 98% H the simple glass sheet to be immersed the Pirhana solution of newly joining
2SO
4Be about 30% H with mass concentration
2O
2Be 7: 3 blended mixed solutions by volume) 5～20 minutes, take out and use distilled water wash, dry up with nitrogen;
(3) sheet glass after step (2) is dried up with nitrogen is immersed in the diallyl dimethyl ammoniumchloride aqueous solution that concentration is 1～3mg/mL and takes out after 2～10 minutes, in glass surface deposition one deck diallyl dimethyl ammoniumchloride coating,, dry up to remove the diallyl dimethyl ammoniumchloride of physical adsorption with distilled water wash with nitrogen; And then immersed in the sodium polystyrene sulfonate aqueous solution that concentration is 1～3mg/mL 2～10 minutes, take out, use distilled water wash, dry up with nitrogen, on the diallyl dimethyl ammoniumchloride coating, deposit one deck sodium polystyrene sulfonate coating again; Repeat the processing step of above-mentioned deposition diallyl dimethyl ammoniumchloride coating and sodium polystyrene sulfonate coating, until being deposited 10 bilayers that constitute by diallyl dimethyl ammoniumchloride coating and sodium polystyrene sulfonate coating altogether, and then repeat the processing step of above-mentioned deposition diallyl dimethyl ammoniumchloride coating, obtain the sheet glass that sedimentary last one deck is the diallyl dimethyl ammoniumchloride coating on sheet glass;
(4) last one deck that step (3) is prepared is that the sheet glass of diallyl dimethyl ammoniumchloride coating is immersed in step (1) and contains the SiO that particle diameter is 10～30nm
2In the suspension of nano spherical particle 2～10 minutes, take out and use distilled water wash, nitrogen dries up, and deposits one deck SiO at the diallyl dimethyl ammoniumchloride coatingsurface
2Nanoparticle layers, and then be immersed in taking-up after 2～10 minutes in the diallyl dimethyl ammoniumchloride aqueous solution that concentration is 1～3mg/mL, at SiO
2Nanoparticle layers surface deposition one deck diallyl dimethyl ammoniumchloride coating, dries up with nitrogen to remove the diallyl dimethyl ammoniumchloride of physical adsorption with distilled water wash; Repeat above-mentioned deposition SiO
2The processing step of nanoparticle layers and deposition diallyl dimethyl ammoniumchloride coating is the SiO of 10～30nm until depositing 9 altogether by particle diameter
2The bilayer that nano spherical particle layer and diallyl dimethyl ammoniumchloride coating constitute, and then repeat above-mentioned deposition SiO
2The processing step of nano spherical particle layer obtains that sedimentary last one deck is that particle diameter is the SiO of 10～30nm on sheet glass
2The sheet glass of nano spherical particle layer;
(5) with step (4) preparation with SiO
2The sheet glass of nanoparticle coating is put into retort furnace, 500～600 degrees centigrade of sintering 2～5 hours, and to remove polyelectrolyte diallyl dimethyl ammoniumchloride and sodium polystyrene sulfonate, the SiO that to obtain by ten layers of particle diameter be 10～30nm
2The surface that the nano spherical particle layer constitutes has the antireflecting coating of coarse structure;
(6) glass substrate of step (5) preparation is put into the polytetrafluoroethylcontainer container of sealing, add an amount of ten trifluoro octyl group Trimethoxy silanes, and the liquid level that makes the ten trifluoro octyl group Trimethoxy silanes that added is lower than the bottom of described glass substrate, in temperature is to make ten trifluoro octyl group Trimethoxy silane thermal evaporations under 100～150 degrees centigrade, ten trifluoro octyl group Trimethoxy silane thermal evaporations are deposited on the above-mentioned anti-reflection coating, finally obtain super-hydrophobicity automatically cleaning anti-reflection coating, it is to be the SiO of 10～30nm by particle diameter
2There are one deck ten trifluoro octyl group Trimethoxy silanes on the surface of the anti-reflection coating that the nano spherical particle layer constitutes, and the surface of ten trifluoro octyl group Trimethoxy silanes has coarse structure.The surface of the anti-reflection coating of described super-hydrophobic automatic cleaning and cross section pattern are as shown in Figure 5.Coat-thickness is about 128nm, and transmittance is shown in Fig. 6 center line 10.Reflectivity is shown in Fig. 7 center line 10.
Embodiment 6
Antireflecting coating: by eight layers of particle diameter SiO that is 30～50nm
2Nanoparticle is formed, its preparation process:
(1) with 3-6mL ammoniacal liquor, the 50-150mL dehydrated alcohol added in the Erlenmeyer flask stirring at normal temperature 8-12 minute, stirred 1-3 minute at 50-70 degree centigrade, under agitation drip 4-6mL tetraethoxy (TEOS), continue to stir 10-14 hour at 50-70 degree centigrade, obtain translucent suspension, gained contains the SiO that diameter is 30～50nm
2Nano spherical particle suspension, and to be diluted to massfraction be that 0.1%～1% suspension is standby;
(2) (mass concentration is about 98% H the simple glass sheet to be immersed the Pirhana solution of newly joining
2SO
4Be about 30% H with mass concentration
2O
2Be 7: 3 blended mixed solutions by volume) 5～20 minutes, take out and use distilled water wash, dry up with nitrogen;
(3) sheet glass after step (2) is dried up with nitrogen is immersed in the diallyl dimethyl ammoniumchloride aqueous solution that concentration is 1～3mg/mL and takes out after 2～10 minutes, in glass surface deposition one deck diallyl dimethyl ammoniumchloride coating,, dry up to remove the diallyl dimethyl ammoniumchloride of physical adsorption with distilled water wash with nitrogen; And then immersed in the sodium polystyrene sulfonate aqueous solution that concentration is 1～3mg/mL 2～10 minutes, take out, use distilled water wash, dry up with nitrogen, on the diallyl dimethyl ammoniumchloride coating, deposit one deck sodium polystyrene sulfonate coating again; Repeat the processing step of above-mentioned deposition diallyl dimethyl ammoniumchloride coating and sodium polystyrene sulfonate coating, until being deposited 15 bilayers that constitute by diallyl dimethyl ammoniumchloride coating and sodium polystyrene sulfonate coating altogether, and then repeat the processing step of above-mentioned deposition diallyl dimethyl ammoniumchloride coating, obtain the sheet glass that sedimentary last one deck is the diallyl dimethyl ammoniumchloride coating on sheet glass;
(4) last one deck that step (3) is prepared is that the sheet glass of diallyl dimethyl ammoniumchloride coating is immersed in step (1) and contains the SiO that particle diameter is 30～50nm
2In the suspension of nano spherical particle 2～10 minutes, take out and use distilled water wash, nitrogen dries up, and deposits one deck SiO at the diallyl dimethyl ammoniumchloride coatingsurface
2Nanoparticle layers, and then be immersed in taking-up after 2～10 minutes in the diallyl dimethyl ammoniumchloride aqueous solution that concentration is 1～3mg/mL, at SiO
2Nanoparticle layers surface deposition one deck diallyl dimethyl ammoniumchloride coating, dries up with nitrogen to remove the diallyl dimethyl ammoniumchloride of physical adsorption with distilled water wash; Repeat above-mentioned deposition SiO
2The processing step of nanoparticle layers and deposition diallyl dimethyl ammoniumchloride coating is the SiO of 30～50nm until depositing 7 altogether by particle diameter
2The bilayer that nano spherical particle layer and diallyl dimethyl ammoniumchloride coating constitute, and then repeat above-mentioned deposition SiO
2The processing step of nano spherical particle layer obtains that sedimentary last one deck is that particle diameter is the SiO of 30～50nm on sheet glass
2The sheet glass of nano spherical particle layer;
(5) with step (4) preparation with SiO
2The sheet glass of nanoparticle coating is put into retort furnace, 500～600 degrees centigrade of sintering 2～5 hours, and to remove polyelectrolyte diallyl dimethyl ammoniumchloride and sodium polystyrene sulfonate, the SiO that to obtain by eight layers of particle diameter be 30～50nm
2The surface that the nano spherical particle layer constitutes has the antireflecting coating of coarse structure;
(6) glass substrate of step (5) preparation is put into the polytetrafluoroethylcontainer container of sealing, add an amount of ten trifluoro octyl group Trimethoxy silanes, and the liquid level that makes the ten trifluoro octyl group Trimethoxy silanes that added is lower than the bottom of described glass substrate, in temperature is to make ten trifluoro octyl group Trimethoxy silane thermal evaporations under 100～150 degrees centigrade, ten trifluoro octyl group Trimethoxy silane thermal evaporations are deposited on the above-mentioned anti-reflection coating, finally obtain super-hydrophobicity automatically cleaning anti-reflection coating, it is to be the SiO of 30～50nm by particle diameter
2There are one deck ten trifluoro octyl group Trimethoxy silanes on the surface of the anti-reflection coating that the nano spherical particle layer constitutes, and the surface of ten trifluoro octyl group Trimethoxy silanes has coarse structure.
Embodiment 7
Antireflecting coating: by 15 layers of particle diameter SiO that is 50～80nm
2Nanoparticle is formed, its preparation process:
(1) with 6-9mL ammoniacal liquor, the 50-150mL dehydrated alcohol added in the Erlenmeyer flask stirring at normal temperature 8-12 minute, stirred 1-3 minute at 50-70 degree centigrade, under agitation drip 3mL tetraethoxy (TEOS), continue to stir 10-14 hour at 50-70 degree centigrade, obtain translucent suspension, gained contains the SiO that diameter is 50～80nm
2Nano spherical particle suspension, and to be diluted to massfraction be that 0.5% suspension is standby;
(2) (mass concentration is about 98% H the simple glass sheet to be immersed the Pirhana solution of newly joining
2SO
4Be about 30% H with mass concentration
2O
2Be 7: 3 blended mixed solutions by volume) 5～20 minutes, take out and use distilled water wash, dry up with nitrogen;
(3) sheet glass after step (2) is dried up with nitrogen is immersed in the diallyl dimethyl ammoniumchloride aqueous solution that concentration is 1～3mg/mL and takes out after 2～10 minutes, in glass surface deposition one deck diallyl dimethyl ammoniumchloride coating,, dry up to remove the diallyl dimethyl ammoniumchloride of physical adsorption with distilled water wash with nitrogen; And then immersed in the sodium polystyrene sulfonate aqueous solution that concentration is 1～3mg/mL 2～10 minutes, take out, use distilled water wash, dry up with nitrogen, on the diallyl dimethyl ammoniumchloride coating, deposit one deck sodium polystyrene sulfonate coating again; Repeat the processing step of above-mentioned deposition diallyl dimethyl ammoniumchloride coating and sodium polystyrene sulfonate coating, until being deposited 15 bilayers that constitute by diallyl dimethyl ammoniumchloride coating and sodium polystyrene sulfonate coating altogether, and then repeat the processing step of above-mentioned deposition diallyl dimethyl ammoniumchloride coating, obtain the sheet glass that sedimentary last one deck is the diallyl dimethyl ammoniumchloride coating on sheet glass;
(4) last one deck that step (3) is prepared is that the sheet glass of diallyl dimethyl ammoniumchloride coating is immersed in step (1) and contains the SiO that particle diameter is 50～80nm
2In the suspension of nano spherical particle 2～10 minutes, take out and use distilled water wash, nitrogen dries up, and deposits one deck SiO at the diallyl dimethyl ammoniumchloride coatingsurface
2Nanoparticle layers, and then be immersed in taking-up after 2～10 minutes in the diallyl dimethyl ammoniumchloride aqueous solution that concentration is 1～3mg/mL, at SiO
2Nanoparticle layers surface deposition one deck diallyl dimethyl ammoniumchloride coating, dries up with nitrogen to remove the diallyl dimethyl ammoniumchloride of physical adsorption with distilled water wash; Repeat above-mentioned deposition SiO
2The processing step of nanoparticle layers and deposition diallyl dimethyl ammoniumchloride coating is the SiO of 50～80nm until depositing 14 altogether by particle diameter
2The bilayer that nano spherical particle layer and diallyl dimethyl ammoniumchloride coating constitute, and then repeat above-mentioned deposition SiO
2The processing step of nano spherical particle layer obtains that sedimentary last one deck is that particle diameter is the SiO of 50～80nm on sheet glass
2The sheet glass of nano spherical particle layer;
(5) with step (4) preparation with SiO
2The sheet glass of nanoparticle coating is put into retort furnace, 500～600 degrees centigrade of sintering 2～5 hours, and to remove polyelectrolyte diallyl dimethyl ammoniumchloride and sodium polystyrene sulfonate, the SiO that to obtain by 15 layers of particle diameter be 50～80nm
2The surface that the nano spherical particle layer constitutes has the antireflecting coating of coarse structure;
(6) glass substrate of step (5) preparation is put into the polytetrafluoroethylcontainer container of sealing, add an amount of ten trifluoro octyl group Trimethoxy silanes, and the liquid level that makes the ten trifluoro octyl group Trimethoxy silanes that added is lower than the bottom of described glass substrate, in temperature is to make ten trifluoro octyl group Trimethoxy silane thermal evaporations under 100～150 degrees centigrade, ten trifluoro octyl group Trimethoxy silane thermal evaporations are deposited on the above-mentioned anti-reflection coating, finally obtain super-hydrophobicity automatically cleaning anti-reflection coating, it is to be the SiO of 50～80nm by particle diameter
2There are one deck ten trifluoro octyl group Trimethoxy silanes on the surface of the anti-reflection coating that the nano spherical particle layer constitutes, and the surface of ten trifluoro octyl group Trimethoxy silanes has coarse structure.
Antireflecting coating: by eight layers of particle diameter SiO that is 80～100nm
2Nanoparticle is formed, its preparation process:
(1) with 3-6mL ammoniacal liquor, the 50-150mL dehydrated alcohol added in the Erlenmeyer flask stirring at normal temperature 8-12 minute, stirred 1-3 minute at 50-70 degree centigrade, under agitation drip 6-9mL tetraethoxy (TEOS), continue to stir 10-14 hour at 50-70 degree centigrade, obtain translucent suspension, gained contains the SiO that diameter is 80～100nm
2Nano spherical particle suspension, and to be diluted to massfraction be that 1% suspension is standby;
(2) (mass concentration is about 98% H the simple glass sheet to be immersed the Pirhana solution of newly joining
2SO
4Be about 30% H with mass concentration
2O
2Be 7: 3 blended mixed solutions by volume) 5～20 minutes, take out and use distilled water wash, dry up with nitrogen;
(3) sheet glass after step (2) is dried up with nitrogen is immersed in the diallyl dimethyl ammoniumchloride aqueous solution that concentration is 1～3mg/mL and takes out after 2～10 minutes, in glass surface deposition one deck diallyl dimethyl ammoniumchloride coating,, dry up to remove the diallyl dimethyl ammoniumchloride of physical adsorption with distilled water wash with nitrogen; And then immersed in the sodium polystyrene sulfonate aqueous solution that concentration is 1～3mg/mL 2～10 minutes, take out, use distilled water wash, dry up with nitrogen, on the diallyl dimethyl ammoniumchloride coating, deposit one deck sodium polystyrene sulfonate coating again; Repeat the processing step of above-mentioned deposition diallyl dimethyl ammoniumchloride coating and sodium polystyrene sulfonate coating, until being deposited 7 bilayers that constitute by diallyl dimethyl ammoniumchloride coating and sodium polystyrene sulfonate coating altogether, and then repeat the processing step of above-mentioned deposition diallyl dimethyl ammoniumchloride coating, obtain the sheet glass that sedimentary last one deck is the diallyl dimethyl ammoniumchloride coating on sheet glass;
(4) last one deck that step (3) is prepared is that the sheet glass of diallyl dimethyl ammoniumchloride coating is immersed in step (1) and contains the SiO that particle diameter is 80～100nm
2In the suspension of nano spherical particle 2～10 minutes, take out and use distilled water wash, nitrogen dries up, and deposits one deck SiO at the diallyl dimethyl ammoniumchloride coatingsurface
2Nanoparticle layers, and then be immersed in taking-up after 2～10 minutes in the diallyl dimethyl ammoniumchloride aqueous solution that concentration is 1～3mg/mL, at SiO
2Nanoparticle layers surface deposition one deck diallyl dimethyl ammoniumchloride coating, dries up with nitrogen to remove the diallyl dimethyl ammoniumchloride of physical adsorption with distilled water wash; Repeat above-mentioned deposition SiO
2The processing step of nanoparticle layers and deposition diallyl dimethyl ammoniumchloride coating is the SiO of 50～80nm until depositing 7 altogether by particle diameter
2The bilayer that nano spherical particle layer and diallyl dimethyl ammoniumchloride coating constitute, and then repeat above-mentioned deposition SiO
2The processing step of nano spherical particle layer obtains that sedimentary last one deck is that particle diameter is the SiO of 80～100nm on sheet glass
2The sheet glass of nano spherical particle layer;
(5) with step (4) preparation with SiO
2The sheet glass of nanoparticle coating is put into retort furnace, 500～600 degrees centigrade of sintering 2～5 hours, and to remove polyelectrolyte diallyl dimethyl ammoniumchloride and sodium polystyrene sulfonate, the SiO that to obtain by eight layers of particle diameter be 80～100nm
2The surface that the nano spherical particle layer constitutes has the antireflecting coating of coarse structure;
(6) glass substrate of step (5) preparation is put into the polytetrafluoroethylcontainer container of sealing, add an amount of ten trifluoro octyl group Trimethoxy silanes, and the liquid level that makes the ten trifluoro octyl group Trimethoxy silanes that added is lower than the bottom of described glass substrate, in temperature is to make ten trifluoro octyl group Trimethoxy silane thermal evaporations under 100～150 degrees centigrade, ten trifluoro octyl group Trimethoxy silane thermal evaporations are deposited on the above-mentioned anti-reflection coating, finally obtain super-hydrophobicity automatically cleaning anti-reflection coating, it is to be the SiO of 80～100nm by particle diameter
2There are one deck ten trifluoro octyl group Trimethoxy silanes on the surface of the anti-reflection coating that the nano spherical particle layer constitutes, and the surface of ten trifluoro octyl group Trimethoxy silanes has coarse structure.
The direct sheet glass of above-mentioned glass substrate as glass window, glass sunroof, glass curtain wall, Household bathroom mirror, windshield, automobile rearview mirror, automobile background glass or eye plate.
Claims (10)
1. anti-reflection coating, it is characterized in that: described anti-reflection coating is to be the SiO of 10～100nm by particle diameter
2The nano spherical particle layer constitutes, and the surface of this anti-reflection coating has coarse structure.
2. the anti-reflection coating of a super-hydrophobic automatic cleaning is characterized in that: the anti-reflection coating of described super-hydrophobic automatic cleaning is to be the SiO of 10～100nm in claim 1 by particle diameter
2There is a layered low-surface energy material on the surface of the anti-reflection coating that the nano spherical particle layer constitutes, and the surface of low surface energy material layer has coarse structure;
Described low surface energy material is selected from a kind of in trifluoro propyl Trimethoxy silane, trifluoro propyl triethoxyl silane, ten trifluoro octyl group Trimethoxy silanes, ten trifluoro octyltri-ethoxysilane, 17 fluorine decyl Trimethoxy silanes, 17 fluorine decyl triethoxyl silanes, ten difluoro heptyl propyl trimethoxy silicanes, the hexafluoro butyl propyl trimethoxy silicane.
3. the preparation method of an anti-reflection coating according to claim 1 is characterized in that, described method may further comprise the steps:
(1) processing substrate is clean, remove surface contaminant;
(2) substrate that obtains after step (1) is dried up with rare gas element is immersed in the aqueous solution of diallyl dimethyl ammoniumchloride that concentration is 1～3mg/mL and takes out after 2～10 minutes, in substrate surface deposition one deck diallyl dimethyl ammoniumchloride coating,, dry up to remove the diallyl dimethyl ammoniumchloride of physical adsorption with distilled water wash with rare gas element; And then be immersed in the sodium polystyrene sulfonate aqueous solution that concentration is 1～3mg/mL 2～10 minutes, take out, use distilled water wash, dry up with rare gas element, on the diallyl dimethyl ammoniumchloride coating, deposit one deck sodium polystyrene sulfonate coating again; Repeat the processing step of above-mentioned deposition diallyl dimethyl ammoniumchloride coating and sodium polystyrene sulfonate coating, until being deposited 5～20 layers of bilayer that constitutes by diallyl dimethyl ammoniumchloride coating and sodium polystyrene sulfonate coating altogether, and then repeat the processing step of above-mentioned deposition diallyl dimethyl ammoniumchloride coating, obtain the substrate that sedimentary last one deck is the diallyl dimethyl ammoniumchloride coating on substrate;
(3) last one deck that step (2) is prepared is that the substrate of diallyl dimethyl ammoniumchloride coating is immersed in and contains the SiO that particle diameter is 10～100nm
2In the alcohol suspension of nano spherical particle 2～10 minutes, take out and use distilled water wash, rare gas element dries up, and deposits one deck SiO at the diallyl dimethyl ammoniumchloride coatingsurface
2The nano spherical particle layer; And then be immersed in taking-up after 2～10 minutes in the diallyl dimethyl ammoniumchloride aqueous solution that concentration is 1～3mg/mL, at SiO
2Nano spherical particle laminar surface deposition one deck diallyl dimethyl ammoniumchloride coating, dries up with rare gas element to remove the diallyl dimethyl ammoniumchloride of physical adsorption with distilled water wash; Repeat above-mentioned deposition SiO
2The processing step of nano spherical particle layer and deposition diallyl dimethyl ammoniumchloride coating, until the last one deck that obtains in step (2) is on the substrate of diallyl dimethyl ammoniumchloride coating, and being deposited 2～14 layers altogether is the SiO of 10～100nm by particle diameter
2The bilayer that nano spherical particle layer and diallyl dimethyl ammoniumchloride coating constitute, and then repeat above-mentioned deposition SiO
2The processing step of nano spherical particle layer obtains that sedimentary last one deck is that particle diameter is the SiO of 10～100nm on substrate
2The substrate of nano spherical particle layer;
(4) outermost layer that step (3) is prepared is SiO
2The substrate of nano spherical particle layer is put into retort furnace, is 500～600 degrees centigrade of following sintering in temperature, to remove polyelectrolyte diallyl dimethyl ammoniumchloride and sodium polystyrene sulfonate, obtains described anti-reflection coating on substrate.
4. preparation method according to claim 3 is characterized in that: the described sintering time of step (4) is 2～5 hours.
5. preparation method according to claim 3 is characterized in that: step (3) is described to contain the SiO that particle diameter is 10～100nm
2The mass concentration of the alcohol suspension of nano spherical particle is 0.1%～1%.
6. preparation method according to claim 3 is characterized in that: described substrate is a sheet glass.
7. preparation method according to claim 6 is characterized in that: described sheet glass is glass window, glass sunroof, glass curtain wall, Household bathroom mirror, windshield, automobile rearview mirror, automobile background glass or eye plate.
8. the preparation method of a super-hydrophobic automatic cleaning anti-reflection coating according to claim 2 is characterized in that:
The substrate that has the anti-reflection coating that any preparation method of claim 3～7 obtains is put into the container of sealing, in container, add the low surface energy material, and the liquid level that makes the low surface energy material that is added is lower than the bottom of described substrate, in temperature is to make the evaporation of low surface energy material under 100～500 degrees centigrade, the hydatogenesis of low surface energy material on the anti-reflection coating that has prepared, is finally obtained super-hydrophobic automatic cleaning anti-reflection coating on substrate;
Described low surface energy material is selected from a kind of in trifluoro propyl Trimethoxy silane, trifluoro propyl triethoxyl silane, ten trifluoro octyl group Trimethoxy silanes, ten trifluoro octyltri-ethoxysilane, 17 fluorine decyl Trimethoxy silanes, 17 fluorine decyl triethoxyl silanes, the ten difluoro heptyl propyl trimethoxy silicanes.
9. preparation method according to claim 8 is characterized in that: described substrate is a sheet glass.
10. preparation method according to claim 9 is characterized in that: described glass is the big window of glass window, glass, glass curtain wall, Household bathroom mirror, windshield, automobile rearview mirror, automobile background glass or eye plate.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101627464A CN102234183A (en) | 2010-04-28 | 2010-04-28 | Anti-reflection coating and super-hydrophobic self-cleaning anti-reflection coating and preparation method thereof |
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|---|---|---|---|
| CN2010101627464A CN102234183A (en) | 2010-04-28 | 2010-04-28 | Anti-reflection coating and super-hydrophobic self-cleaning anti-reflection coating and preparation method thereof |
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